摘要
目的建立脂肪酸含量测定的高效液相色谱法,并以此测定鸦胆子油乳注射液中的游离脂肪酸和结合脂肪酸含量。方法用ω-溴代苯乙酮为衍生化试剂,三乙醇胺为催化剂对脂肪酸进行酯化使其产生紫外吸收,利用HPLC法进行分离定量。色谱条件为:采用Shim-packVP-ODS(C18,150L×4.6mm,5μm)色谱柱,检测波长242nm,流动相为甲醇∶乙腈∶H2O=65∶27∶8,柱温:25℃,流速1.0mL/min。十七烷酸为内标。结果在上述色谱条件下,各脂肪酸衍生物均达到基线分离。鸦胆子油乳注射液中游离脂肪酸含量较低,主要为结合脂肪酸。结论本方法为评价和控制鸦胆子油乳质量提供了依据。
OBJECTIVE To determine the contents of fatty acids in Brucea jananica oil injection by high-performance liquid chromatography. METHODS The fatty acids in Brucea jananica oil injection were saponified and esterified to esters with ω-bromophenacyl bromide. Phenacyl bromide esters of fatty acids in Brucea jananica oil injection were best resolved using an octadecylsilyl column with endcapped silanol groups. An isocratie elution method using methanol-acetonitrile water （65： 28： 7） at 1 mL/min with UV detection at 242 nm and a column temperature of 25℃ was found to optimally resolve the four major fatty acids present in Bruceajananica oil （ palmitic acid [ 16： 0], stearic [ 18： 0], oleic [ 18：1 ] and linoleic [ 18： 2] ）, with a run time of less than 45 min. The entire process including pre-column derivatization, and HPLC quantitation can be completed in 120 min. RESULTS Established techniques for fatty acid derivatization and HPLC separation. CONCLUSION The method is rapid, sensitive and highly reproducible. It is suitable for the determination of fatty acids in Brucea jananica oil injection.
出处
《中国现代应用药学》
CAS
CSCD
北大核心
2006年第4期329-331,共3页
Chinese Journal of Modern Applied Pharmacy
基金
广东省中医药局2004年度科研课题
课题编号:1040073
关键词
鸦胆子油乳注射液
脂肪酸
含量测定
Brucea jananica oil
fatty acid
quantification determination
